Dimethyl Carbonate → Lithium phosphorodifluoridate

HRID 1499992

Reaction equation

HRID 1499992 reaction equation
[P:1]([F:5])([F:4])(=[O:3])[OH:2].F[P-](F)(F)(F)(F)F.[Li+:13].[Cl-].[Mg+2:15].[Cl-].C(=O)(OC)OC>>[P:1]([F:5])([F:4])([O-:3])=[O:2].[Mg+2:15].[P:1]([F:5])([F:4])([O-:3])=[O:2].[P:1]([F:5])([F:4])([O-:3])=[O:2].[Li+:13]

Participants

6

Reactant 4

HCID 12021Dimethyl CarbonateHCID 61681Difluorophosphoric acidHCID 5360315Magnesium ChlorideHCID 23688915Lithium hexafluorophosphate

Product 2

HCID 23697195Lithium phosphorodifluoridateHCID 86653259Magnesium difluorophosphate

Conditions

Temperature
130 °C

Procedure

Difluorophosphoric acid (reagent, produced by Fluorochem Ltd.) (15.4 g) was weighed into a 250 ml-volume PFA vessel, and 3.4 g of lithium hexafluorophosphate (reagent, produced by Stella Chemifa Corporation) was added. Furthermore, 7.1 g of magnesium chloride (reagent, produced by Wako Pure Chemical Industries, Ltd.) and 15.0 g of dimethyl carbonate (reagent, produced by Kishida Chemical Co., Ltd.) were added, and the mixture was stirred for 1 hour under nitrogen flow and after heating at 130° C. for 17 hours, cooled to room temperature to obtain a mixed crystal of magnesium difluorophosphate and lithium difluorophosphate. Anion analysis was performed in the same manner as in Example 2-6, as a result, the obtained difluorophosphate ion was 91% in terms of the relative area.

Workup

  1. additionwas added
  2. temperaturecooled to room temperature

Sources & evidence

ORD record
ord-2d1c14e66aef4fe58ba858170288f5c2
Source dataset
uspto-grants-2015_12
Patent number
US09203106B2

Linked notes

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